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Speciation of Manganese in a Synthetic Recycling Slag Relevant for Lithium Recycling from Lithium-Ion Batteries

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Speciation of Manganese in a Synthetic Recycling Slag Relevant for Lithium Recycling from Lithium-Ion Batteries metals Article Speciation of Manganese in a Synthetic Recycling Slag Relevant for Lithium Recycling from Lithium-Ion Batteries Alena Wittkowski 1, Thomas Schirmer 2, Hao Qiu 3 , Daniel Goldmann 3 and Ursula E. A. Fittschen 1,* 1 Institute of Inorganic and Analytical Chemistry, Clausthal University of Technology, Arnold-Sommerfeld Str. 4, 38678 Clausthal-Zellerfeld, Germany; [email protected] 2 Department of Mineralogy, Geochemistry, Salt Deposits, Institute of Disposal Research, Clausthal University of Technology, Adolph-Roemer-Str. 2A, 38678 Clausthal-Zellerfeld, Germany; [email protected] 3 Department of Mineral and Waste Processing, Institute of Mineral and Waste Processing, Waste Disposal and Geomechanics, Clausthal University of Technology, Walther-Nernst-Str. 9, 38678 Clausthal-Zellerfeld, Germany; [email protected] (H.Q.); [email protected] (D.G.) * Correspondence: ursula.fi[email protected]; Tel.: +49-5323-722205 Abstract: Lithium aluminum oxide has previously been identified to be a suitable compound to recover lithium (Li) from Li-ion battery recycling slags. Its formation is hampered in the presence of high concentrations of manganese (9 wt.% MnO2). In this study, mock-up slags of the system Li2O-CaO-SiO2-Al2O3-MgO-MnOx with up to 17 mol% MnO2-content were prepared. The man- ganese (Mn)-bearing phases were characterized with inductively coupled plasma optical emission spectrometry (ICP-OES), X-ray diffraction (XRD), electron probe microanalysis (EPMA), and X-ray absorption near edge structure analysis (XANES). The XRD results confirm the decrease of LiAlO2 phases from Mn-poor slags (7 mol% MnO2) to Mn-rich slags (17 mol% MnO2). The Mn-rich grains are predominantly present as idiomorphic and relatively large (>50 µm) crystals. XRD, EPMA and XANES suggest that manganese is present in the form of a spinel solid solution. The absence of light Citation: Wittkowski, A.; Schirmer, T.; elements besides Li and O allowed to estimate the Li content in the Mn-rich grain, and to determine Qiu, H.; Goldmann, D.; Fittschen, U.E.A. 2+ 3+ a generic stoichiometry of the spinel solid solution, i.e., (Li(2x)Mn (1−x))1+x(Al(2−z),Mn z)O4. The Speciation of Manganese in a coefficients x and z were determined at several locations of the grain. It is shown that the aluminum Synthetic Recycling Slag Relevant for x z Lithium Recycling from Lithium-Ion concentration decreases, while the manganese concentration increases from the start ( : 0.27; : 0.54) Batteries. Metals 2021, 11, 188. to the end (x: 0.34; z: 1.55) of the crystallization. https://doi.org/10.3390/met11020188 Keywords: lithium; engineered artificial minerals (EnAM); X-ray absorption near edge structure Academic Editor: Mark E. Schlesinger (XANES); powder X-ray diffraction (PXRD); electron probe microanalysis (EPMA); melt experiments Received: 30 December 2020 Accepted: 18 January 2021 Published: 21 January 2021 1. Introduction Publisher’s Note: MDPI stays neutral Modern technologies, such as renewable energy and e-mobility, demand a new port- with regard to jurisdictional claims in folio of technology-critical elements and materials. Limited resources, national policies or published maps and institutional affil- monopolies threaten the supply of some technology-critical elements. Hence, the recovery iations. of these elements from waste is crucial. On the one hand, demand for lithium (Li) has increased rapidly due to the popularity and extraordinary performance of Li-ion batteries. On the other hand, Li is produced by mainly two countries, Australia (ca. 55%) and Chile (ca. 23%) [1]. The recycling of some components from Li-ion batteries is already put into Copyright: © 2021 by the authors. practice, e.g., cobalt, in a pyrometallurgical process [2,3]. Pyrometallurgical recycling has Licensee MDPI, Basel, Switzerland. the benefit of being adaptable to many waste streams; additionally, the emission of toxic This article is an open access article compounds like HF is prevented. Due to its ignoble character, Li is driven into the slag and distributed under the terms and is usually not recovered.The recovery of Li from pyrometallurgical recycling slags can be conditions of the Creative Commons accomplished by the targeted formation of “engineered artificial minerals” (EnAM). Attribution (CC BY) license (https:// The strategy of EnAM formation is to concentrate the elements of interest in a few creativecommons.org/licenses/by/ phases, with a structure and size that allows an efficient separation. Figure1 shows a 4.0/). Metals 2021, 11, 188. https://doi.org/10.3390/met11020188 https://www.mdpi.com/journal/metals Metals 2021, 11, x FOR PEER REVIEW 2 of 22 can be accomplished by the targeted formation of “engineered artificial minerals” (EnAM). Metals 2021, 11, 188 2 of 20 The strategy of EnAM formation is to concentrate the elements of interest in a few phases, with a structure and size that allows an efficient separation. Figure 1 shows a schemescheme of EnAM of EnAM formation. formation. The The target target element elemen (yellowt (yellow triangle) triangle) spreads spreads over over severalseveral dif- differentferent phases phases (red (red and and green green forms) forms) and and the the matrix matrix (blue) (blue) in thein the unmodified unmodified slag slag (top (top picture).picture). The The target target element element will will be be difficult difficult to to isolate isolate due due to to itsits occurrenceoccurrence inin many dif- differentferent phases. phases. The The goal goal in in EnAM EnAM isis toto concentrateconcentrate thethe targettarget element in a single phase (red (redpentagon, pentagon, bottom picture)picture) that that differs differs physically physically and and chemically chemically from from the the other other phases phases (green(green hexagon), hexagon), and and allows allows for efficient for efficient separation separation and furtherand further treatment. treatment. Figure 1. Sketch of engineered artificial minerals (EnAM) formation. On the left, different elements are shown in the liquid Figure 1. Sketch of engineered artificial minerals (EnAM) formation. On the left, different elements are shown in the liquid slag-matrix:slag-matrix: target target element element (yellow (yellow triangle), triang phasele), phase for EnAM for EnAM (red) (red) and otherand other phases phases (green). (green). The upperThe upper route route refers refers to an to an unmodifiedunmodified slag–the slag–the target target element element is spread is spread over over several several different different phases phases and theand matrix the matrix (blue). (blu Thee). targetThe target element element is not is not recovered.recovered. The bottomThe bottom picture picture illustrates illustrates the formation the formation of EnAM. of EnAM. The targetThe target element element is concentrated is concentrated in a singlein a single phase phase (red (red pentagon)pentagon) that differsthat differs physically physically and chemicallyand chemically from from the other the othe phasesr phases (green (green hexagon), hexagon), and allowsand allows for efficient for efficient separation separation and furtherand further treatment. treatment. Separation of artificial minerals, enriched in valuable elements from remaining slag Separation of artificial minerals, enriched in valuable elements from remaining slag components, might be carried out by flotation processes. Here, the composition and struc- components, might be carried out by flotation processes. Here, the composition and struc- ture of phases are crucial. It can be expected that none of the artificially produced minerals ture of phases are crucial. It can be expected that none of the artificially produced minerals will show hydrophobic behavior by nature. Thus, the mineral-collector-interaction has to will show hydrophobic behavior by nature. Thus, the mineral-collector-interaction has to be studied, and this interaction relies strongly on crystal structure and ions, responsible for be studied, and this interaction relies strongly on crystal structure and ions, responsible the adsorption of the active group of collector molecules. for the adsorption of the active group of collector molecules. The recovery of Li from slags has been subject to several studies. Elwert et al. [2] found The recovery of Li from slags has been subject to several studies. Elwert et al. [2] that Li reacts with aluminum to form predominately large lithium aluminate (LiAlO2) crystals.found The that aluminum Li reacts binds with Li aluminum from the melt to form uniformly predominately in one phase large at an lithium early state aluminate of solidifying(LiAlO phase2) crystals. of the The molten aluminum slag. The binds idiomorphic Li from the to melt hypidiomorphic uniformly in lithium one phase aluminate at an early crystalsstate can of solidifying easily be separated phase of from the molten the matrix slag. by The flotation. idiomorphic Hence, to lithium hypidiomorphic aluminate islithium a aluminate crystals can easily be separated from the matrix by flotation. Hence, lithium promising EnAM candidate. The recovery of Li from LiAlO2 was successfully conducted by Haasaluminate et al. [is4 ].a Elwertpromising et al. EnAM [5] investigated candidate. The a hydrometallurgical recovery of Li from process LiAlO to2 was recover success- Li fromfully slags conducted with low by aluminumHaas et al. compared[4]. Elwert toet [al.2] [5] and investigated enriched in a silicone. hydrometallurgical However, it pro-
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